Yield:-

Reaction Conditions:

with triethylamine in water at 42;Inert atmosphere;

Steps:

1
Example1:PreparationofamorphousoxamylinaccordancewiththedisclosureofUSPAT.NO.5,284,962,Example2Atwo-stage,co-currentlyfed,continuousreactorsystemwasusedtoreactMIC(methylisocyanate)andtheoxime,methyl2-(dimethylamino)-N-hydroxy-2-oxoethanimidothioate,toproducemethyl2-(dimethylamino)-N-[[(methylamino)carbonyl]oxy]-2-oxoethanimidothioate(oxamyl).Thereactorsweremaintainedatapproximately42.Duringsteadystateoperation,methylisocyanate(MIC)wasfedatarateof1.2g/minandvaporizedandmixedwithnitrogenwhichwasfedatapproximately2200mL/min.Theoximewasfedatarateof7.9g/minasa40slurryinwatercontaining0.2TEA.Conversionoftheoximeinthefirstreactorwasabout93.Thecompositionoftheproductsolutionfromthesecondreactorwasapproximately47titleproduct,0.9oximeand0.8DMU(dimethylurea).Thiscompositioncorrespondedto97conversionoftheoximeand8oftheoriginalMICasDMU.Theventstreamfromthesecondreactorcontainedabout0.2MICcorrespondingtoremovalofgreaterthan99fromthegasstream.AsshowninFigure4,theX-raypowderdiffractionpatternoftheresultingoxamylproducthasnosignificantsignals,whichindicatestheoxamylproductpreparedinaccordancewiththedisclosureofUSPAT.NO.5,284,962isamorphous.

References:

JIANGSU ROTAM CHEMISTRY CO., LTD.;BRISTOW, James, Timothy WO2018/99203, 2018, A1 Location in patent:Page/Page column 14-15

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